Formation of nitrates of metallic elements



April 1934- H. B. KIPPER FORMATION OF NITRATES OF METALLIC ELEMENTS INVENTOR.

Filed Sept. 14, 1928 ATTORNEYS.

UNITED STATES PATENT OFFICE FORMATION OF NITRATES OF METALLIC ELEMENTS Herman B. Kipper, Cleveland, Ohio, assignor to R. Baylor Knox, Bronxville, N. Y.

Application September 14, 1928, Serial No. 306,078

4 Claims. (01. 23-102) The present invention relates to the formation block or carriage 16 of metal or like material by of the nitrates of the alkali metals, of the alkali means of holding pins 17 which frictionally enearth metals and of other metals, from their gage in recesses in the bomb 10, or by any other oxides, or other compounds or the metals themcommon holding means. The holding block or selves, by the action of nitrogen and oxygen at carriage 16 itself, which has a recessed portion super atmospheric or very high pressures and into which the bomb fits, and a passageway temperature. therethrough for the passage of the pipe .13, is The prime object of the invention is to provide similarly held in position by holding pins 18 a simple effective manner of performing the mounted through the sides of the external 10 conversion. housing. 6.

I have found for example, that if calcium A removable top is provided for the housing oxide first heated to 1000" C. or above is placed to permit access to the bomb l0 and an opening in a closed metallic insulated vessel and subprovided at the bottom of said housing for the V jected to the action of oxygen and nitrogen or passage of pipe 13 therethrough. 5 ordinary air, under a pressure of 100 atmospheres The pipe 13 is connected to a gas feed line 19 or above, the vessel meanwhile conducting off or which may be connected to a suitable gas cylinradiating away the heat of the action, (the rate der 20 containing the gases necessary in the reof conduction or radiation being not too rapid action. Said line 19 has connected in it a presand limited by internal insulation) that on sure gauge 21, a valve 22, a release valve 23 and N 20 cooling, the calcium oxide is largely converted to release opening 23'. Of course more than one calcium nitrate. The chemical reaction involved source of gas supply may exist. For instance I being symbolically expressed as follows: may have several separate tanks each containing one of the gases necessary for my process all CaO+N2+5OTCMNOW leading to the common gas inlet 13 as will be 25 or if we desire to write the equation according readily understood by those skilled in the art. 89 to the more common conception of molecular In carrying out my process, first the element or quantities, as follows: oxide or other compound of the metallic element of which it is desired to make the nitrate, for in- 2CaO+2N2+502- 2Ca(NO3)2 stance calcium oxide or lime, in this instance M The gases in question used are somewhat in lime, in very finely divided form is heated to over 3 excess quantities or in equivalents to that actual- 1200 C. after which it is quickly inserted into the ly required by the reaction involved. bomb 10 through the top thereof and the stopper My process will be more clearly understood 11 immediately put in place, then a mixture of with reference to the drawing which is part of the oxygen and nitrogen, in about the proportioning specification and in which similar references deof 1:4 or approximately in the proportion in which note corresponding parts; Fig. l is a partial cross they are contained in air, and at about 2000 lbs. sectional front elevation of one form of device pressure, is admitted into the bomb through the necessary for my process and Fig. 2 is a similar pipe 13. The contents are then allowed to cool view of a modified form of my apparatus. for a few hours, the rate of cooling being deter- 0 The reactioning or processing is carried out in mined by the insulating capsule 14, and then the i a bomb 10 of steel or other suitable material bomb is opened. Upon testing of the resulting having a removable closure member 11 at one end product in the bomb as by treating with hot water and which may be screw threaded or otherwise and determining the unconverted or free lime, it removably positioned, and having a similar 010- is found that approximately of the contents of sure member 12 at the other end provided with the bomb has been converted to the nitrate. With 9 a gas inlet pipe 13 passing therethrough for a higher gas pressures it would seem reasonable to purpose hereinafter specified. Suitably mountbelieve from the law of mass reaction, that the ed in the interior of the bomb is a capsule of percentage conversionmight be greatly raised and insulating material 14 such as asbestos or the possibly made almost quantitative. 0 like which has been saturated with or used as a I have tried my process with mixtures of co-m- 5" carrier for platinum black which acts as a catapounds of the metallic elements such as mixtures lyst in my process. of calcium oxide with potassium and sodium hy- The bomb 10 is suitably mounted within an droxide and have secured similar results. external safety nipple or housing 15 of suitable The necessity of the presence of the catalyst, material such as steel or the like, on a holding platinum black, on the asbestos capsule is still an 11 undetermined factor but I do know that the process is readily performed in its presence.

The dimensions of the bomb of course may be any size and limited only by the engineering difficulties involved where high pressure and temperature are used. In one form as used by myself the steel bomb was about four inches long, four inches in external diameter and having walls one and one quarter inches thick.

In another modification shown in Fig. 2 I disclose the possibility of the use of an electric arc in the reaction chamber above the lime or other compound to be converted to its nitrate whereby the preheating of the metallic compound may be made far less intensive or done away with entirely.

The apparatus designed for carrying out the processing for nitrate formation in which an electric arc is used in the reactioning, as shown in Fig. 2 is briefly as follows:

25 is a heavy walled reaction vessel of steel or other metal with end closing plugs 26 and 27 screw threadedly or otherwise removably mounted therein, the latter having tapered or funnel like openings in which water cooled electrodes 28 and 29 are mounted on tapered blocks 30 and 31 respectively, insulated from the plugs 26 and 27 by suitable insulating material 32, said electrodes being mounted nearer the top of my device so as to allow ample room below them for the material which is to be converted to the nitrate. The vessel 25 is internally insulated by means of a suitable insulating capsule 38 suitably impregnated with a catalyst such as platinum black and is also provided with a gas inlet pipe 34 leading to a source of gas supply similar to that shown in Fig. l. The compounds in the lower part of the vessel are not directly in the path of the are. It is essential in order that decomposition of nitrate as formed may not take place, to hold the temperature thereof below that of decomposition under the condition of operation, that is the decomposition temperature is in equilibrium with the temperature of the gases at the specific super-atmospheric pressure of operation, and this is done by keeping the compound in the lower path of the vessel out of the direct path of the arc.

In performing the process with this last named device the oxide or other compound of the metal to be converted to the nitrate which may be either highly preheated, or slightly so, or cold, and in finely divided form, is placed in the lower part of the vessel. The stoppers are then closed and gas consisting as before of a mixture of nitrogen and oxygen in the same or about the same ratio and at the same pressure as in the first named process is admitted through the inlet 34.. A high tension arc is then struck between the electrodes 28 and 29 as for instance by applying a high over voltage or else by mechanical means. This are preheats the gases which then come in contact with the compound for instance lime or calcium oxide in the lower region of the tank and convert it to the nitrate as before.

I of course do not wish to confine myself to any fixed temperatures or pressures, nor do I wish to confine myself to any specific element of metal. For instance a larger proportion of oxygen and gas mixture than that used by me may be of advantage. Then again the use of the high pressure gases previously preheated for instance by passing them from one conversion chamber to another may be found to be of advantage. If excess preheated gas is used the uncombined heated gases may be led off from the reaction chamber by suitable means and the pressure and heat thereof used in carrying on or initiating the reaction in other similar chambers or else for preheating gas to be passed into the existing reaction chamber.

If the heat of reaction for formation of the mtrate is negative, external heating might of course be advantageous.

It is obvious that my process may be modified Without departing from the spirit of my invention and I do not wish to be limited by the details shown and described.

Of course the other catalysts such as copper oxide, iron oxide, vanadium oxide, combinations thereof, or other similar materials may be substituted for platinum black.

What I claim is:

1. In a process for the formation of the nitrate, of alkali earth elements, the step of subjecting the oxides of said metals which are in finely divided form and are heated to a high temperature but below their fusion points, to the action of nitrogen and oxygen gases at a pressure of 100 atmospheres or above, whereby the nitrates of said elements are formed.

2. In a process for the formation of calcium nitrate the steps of heating calcium oxide to 1000 C. of enclosing the same while still heated in a metallic vessel internally insulated and of subjecting the same to oxygen and nitrogen at at least 100 atmospheres pressure, whereby calcium nitrate is formed.

3. In a process for the formation of calcium nitrate, the steps of first heating finely divided calcium oxide to approximately 1200" C., then treating said finely divided calcium oxide while at said temperature and in the presence of a catalytic agent with a mixture of uncombined oxygen and nitrogen gas in the ratio for the formation of calcium nitrate and above 2000 pounds pressure to form calcium nitrate.

4. In a process for the formation of calcium nitrate, the step of treating in the presence of catalytic agent finely divided calcium oxide with uncombined oxygen and nitrogen in the ratio for the formation of calcium nitrate and at above 2000 pound pressure under high temperature.

HERMAN B. KIPPER. 

